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Experiments are described, where by deposition of Ni from a Knudsen‐type effusion cell in an O2 atmosphere onto an Au(111) substrate epitaxial and ordered NiO layers are formed. By analyzing the surfaces with scanning tunneling microscopy (STM) and low‐energy electron diffraction (LEED) it is found for room temperature condensation a three‐domain NiO(100) film, while for deposition on a heated (300 °C) substrate NiO(111) is obtained. In the latter case three‐dimensional NiO(111) crystallites and a thin smooth NiO(111) structure showing a p(2 × 2) reconstruction is observed. A p(2 × 2) reconstruction is theoretically expected, if the surface is composed of octopolar subunits ((NiO)4), which overcomes the problem of Madelung instability of a polar surface.

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